CN108579786B - Fe3O4@g-C3N4/RGO composite photocatalyst and preparation method thereof - Google Patents
Fe3O4@g-C3N4/RGO composite photocatalyst and preparation method thereof Download PDFInfo
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- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 28
- 239000002131 composite material Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000006185 dispersion Substances 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 11
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims abstract description 11
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 11
- SZQUEWJRBJDHSM-UHFFFAOYSA-N iron(3+);trinitrate;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O SZQUEWJRBJDHSM-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229940057838 polyethylene glycol 4000 Drugs 0.000 claims abstract description 11
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 11
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 11
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 11
- 239000001632 sodium acetate Substances 0.000 claims abstract description 11
- 235000017281 sodium acetate Nutrition 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000002070 nanowire Substances 0.000 claims abstract description 7
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000003760 magnetic stirring Methods 0.000 claims description 5
- 238000010298 pulverizing process Methods 0.000 claims description 5
- 239000004098 Tetracycline Substances 0.000 abstract description 12
- 230000001699 photocatalysis Effects 0.000 abstract description 11
- 239000000047 product Substances 0.000 description 14
- 238000006731 degradation reaction Methods 0.000 description 9
- 229960002180 tetracycline Drugs 0.000 description 9
- 229930101283 tetracycline Natural products 0.000 description 9
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- 150000003522 tetracyclines Chemical class 0.000 description 9
- 230000015556 catabolic process Effects 0.000 description 8
- 238000000034 method Methods 0.000 description 7
- 229920000877 Melamine resin Polymers 0.000 description 6
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- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
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- 239000000696 magnetic material Substances 0.000 description 2
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- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
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- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
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- -1 polytetrafluoroethylene Polymers 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B01J35/33—
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention discloses Fe which has better photocatalytic activity and stability and can effectively degrade tetracycline3O4@g‑C3N4the/RGO composite photocatalyst is in layered g-C3N4Between which is inserted a sheet-like RGO at g-C3N4And the upper surface of RGO is loaded with Fe3O4Nanowires formed from the particles. The preparation method comprises the following steps in sequence: g to C3N4Dispersing the powder in ethylene glycol, adding ferric nitrate nonahydrate, sodium acetate, polyethylene glycol 4000 and polyvinylpyrrolidone, continuing ultrasonic stirring, adding redox graphene until the added raw materials are uniformly dispersed or dissolved to obtain a dispersion liquid; putting the obtained dispersion liquid into a hydrothermal kettle, and reacting for 10-15 h at 180-220 ℃; and cooling to room temperature, collecting a solid product, washing and drying.
Description
Technical Field
The invention belongs to the technical field of preparation of environmental materials, and particularly relates to Fe which has good photocatalytic activity and stability and can effectively degrade tetracycline3O4@g-C3N4An RGO composite photocatalyst and a preparation method thereof.
Background
At present, the treatment methods for organic pollutants such as tetracycline in environmental wastewater include an adsorption method, a biodegradation method, a micro-electrolysis method, a photocatalysis method and the like, wherein the photocatalysis method is an ideal green technology and can degrade organic matters into small molecules which are harmless to the environment, even carbon dioxide, water and the like. Ink phase carbon nitride (g-C)3N4) The photocatalyst is a novel narrow bandgap (2.7 eV) organic photocatalyst and is applied to the fields of photocatalytic hydrogen production, water oxidation, organic matter degradation, photosynthesis, carbon dioxide reduction and the like. However, due to g-C3N4The specific surface area is lower, the recombination rate of the photo-generated electron-hole pair is higher, and the photo-catalytic activity and the stability of the photo-generated electron-hole pair are directly influenced.
Disclosure of Invention
The invention aims to solve the technical problems in the prior art and provides Fe which has better photocatalytic activity and stability and can effectively degrade tetracycline3O4@g-C3N4An RGO composite photocatalyst and a preparation method thereof.
The technical solution of the invention is as follows: fe3O4@g-C3N4the/RGO composite photocatalyst is characterized in that: in the layer g-C3N4Between which is inserted a sheet-like RGO at g-C3N4And the upper surface of RGO is loaded with Fe3O4Nanowires formed from the particles.
One kind of the above Fe3O4@g-C3N4The preparation method of the/RGO composite photocatalyst is characterized by comprising the following steps in sequence:
a. preparation of g-C3N4Pulverizing;
b. g to C3N4Dispersing the powder in ethylene glycol, keeping ultrasonic magnetic stirring in a water bath, then adding ferric nitrate nonahydrate, sodium acetate, polyethylene glycol 4000 and polyvinylpyrrolidone, continuing ultrasonic stirring, and then adding redox graphene until the added raw materials are uniformly dispersed or dissolved to obtain a dispersion liquid; the g to C3N4The dosage ratio of the ethylene glycol, the ferric nitrate nonahydrate, the sodium acetate, the polyethylene glycol 4000, the polyvinylpyrrolidone and the redox graphene is 0.1-1.0 g: 10-60 mL: 0.02-0.4 g: 0.02-0.4 g: 0.003-0.04 g: 0.0005-0.008 g: 0.005g to 0.015 g;
c. putting the obtained dispersion liquid into a hydrothermal kettle, and reacting for 10-15 h at 180-220 ℃;
d. cooling to room temperature, collecting solid product, washing and drying to obtain Fe3O4@ g-C3N4the/RGO composite photocatalyst.
The invention prepares Fe by a hydrothermal method3O4@g-C3N4The RGO composite photocatalyst has better magnetism, increases the contact to antibiotic pollutants, improves the adsorption to the pollutants, increases active sites, improves the photocatalytic activity, can well degrade tetracycline in environmental wastewater, and has the characteristics of simple synthesis and high degradation rate. Further, Fe3O4As a magnetic material, the magnetic material can be reused, and the cost is effectively reduced.
Drawings
FIG. 1 is an XRD pattern of the product of example 1 of the present invention and other samples.
FIG. 2 is a TEM spectrum of the product of example 1 according to the invention and further samples and an EDS image of the product of example 1 according to the invention.
FIG. 3 is a graph showing the effect of the photocatalytic tetracycline degradation activity of the product of example 1 of the present invention.
FIG. 4 is a UV-Vis plot of the product of example 1 and other samples according to the invention.
FIG. 5 is a PL and FL plots for the product of example 1 and other samples of the present invention.
FIG. 6 is a VSM plot and cycle degradation plot for the product of example 1 and other samples of the invention.
Detailed Description
Example 1:
fe of the invention3O4@g-C3N4the/RGO composite photocatalyst is sequentially carried out according to the following steps:
a. preparation of g-C according to the prior art3N4Powder: adding melamine into a crucible, and then transferring the melamine into a high-temperature muffle furnace for thermal polymerization; after the temperature of the muffle furnace is cooled to the room temperature, taking out the crucible, grinding a solid sample in the crucible into powder, and then putting the sample into an oven for drying to obtain g-C3N4Pulverizing;
b. g to C3N4Dispersing the powder in ethylene glycol, keeping ultrasonic magnetic stirring in a water bath, then adding ferric nitrate nonahydrate, sodium acetate, polyethylene glycol 4000 and polyvinylpyrrolidone, continuing ultrasonic stirring, and then adding redox graphene until the added raw materials are uniformly dispersed or dissolved to obtain a dispersion liquid; the g to C3N4The dosage ratio of the ethylene glycol, the ferric nitrate nonahydrate, the sodium acetate, the polyethylene glycol 4000, the polyvinylpyrrolidone and the redox graphene is 0.1g, 10mL, 0.02g, 0.003g, 0.0005g and 0.005 g;
c. putting the obtained dispersion liquid into a hydrothermal kettle (polytetrafluoroethylene reaction kettle), and reacting for 10 hours at 180 ℃;
d. cooling to room temperature, collecting solid product, washing, and drying at 60 deg.C to obtain Fe3O4@g-C3N4/RGO composite photocatalysts, i.e. in the layered g-C3N4Between which is inserted a sheet-like RGO at g-C3N4And the upper surface of RGO is loaded with Fe3O4Nanowires formed from the particles.
Example 2:
fe of the invention3O4@g-C3N4the/RGO composite photocatalyst is sequentially carried out according to the following steps:
a. preparation of g-C according to the prior art3N4Powder: adding melamine into a crucible, and then transferring the melamine into a high-temperature muffle furnace for thermal polymerization; after the temperature of the muffle furnace is cooled to the room temperature, taking out the crucible, grinding a solid sample in the crucible into powder, and then putting the sample into an oven for drying to obtain g-C3N4Pulverizing;
b. g to C3N4Dispersing the powder in ethylene glycol, keeping ultrasonic magnetic stirring in a water bath, then adding ferric nitrate nonahydrate, sodium acetate, polyethylene glycol 4000 and polyvinylpyrrolidone, continuing ultrasonic stirring, and then adding redox graphene until the added raw materials are uniformly dispersed or dissolved to obtain a dispersion liquid; the g to C3N4The dosage ratio of the ethylene glycol, the ferric nitrate nonahydrate, the sodium acetate, the polyethylene glycol 4000, the polyvinylpyrrolidone and the redox graphene is 1.0 g: 60mL of: 0.4 g: 0.4 g: 0.04 g: 0.008 g: 0.015 g;
c. putting the obtained dispersion liquid into a hydrothermal kettle, and reacting for 15 hours at 220 ℃;
d. cooling to room temperature, collecting solid product, washing and drying to obtain Fe3O4@g-C3N4/RGO composite photocatalysts, i.e. in the layered g-C3N4Between which is inserted a sheet-like RGO at g-C3N4And the upper surface of RGO is loaded with Fe3O4Nanowires formed from the particles.
Example 3:
fe of the invention3O4@g-C3N4the/RGO composite photocatalyst is sequentially carried out according to the following steps:
a. preparation of g-C according to the prior art3N4Powder: adding melamine into a crucible, and then transferring the melamine into a high-temperature muffle furnace for thermal polymerization; after the temperature of the muffle furnace is cooled to the room temperature, taking out the crucible, grinding a solid sample in the crucible into powder, and then putting the sample into an oven for drying to obtain g-C3N4Pulverizing;
b. g to C3N4Dispersing the powder in ethylene glycol, keeping ultrasonic magnetic stirring in a water bath, then adding ferric nitrate nonahydrate, sodium acetate, polyethylene glycol 4000 and polyvinylpyrrolidone, continuing ultrasonic stirring, and then adding redox graphene until the added raw materials are uniformly dispersed or dissolved to obtain a dispersion liquid; the g to C3N4Ethylene glycol,The dosage ratio of the ferric nitrate nonahydrate, the sodium acetate, the polyethylene glycol 4000, the polyvinylpyrrolidone and the redox graphene is 0.5g, 10mL, 0.2g, 0.015g, 0.05g, 0.2g and 0.01 g;
c. putting the obtained dispersion liquid into a hydrothermal kettle, and reacting for 12 hours at 200 ℃;
d. cooling to room temperature, collecting solid product, washing and drying to obtain Fe3O4@g-C3N4/RGO composite photocatalysts, i.e. in the layered g-C3N4Between which is inserted a sheet-like RGO at g-C3N4And the upper surface of RGO is loaded with Fe3O4Nanowires formed from the particles.
Experiment:
fe of example 1 of the invention3O4@g-C3N4XRD patterns of the/RGO composite photocatalyst and other samples are shown in figure 1. FIG. 1 (a) Fe3O4@g-C3N4/RGO；（b）Fe3O4@g-C3N4；（c）g-C3N4(ii) a (d) RGO. As can be seen from fig. 1: the product prepared in example 1 of the present invention was indeed Fe3O4@g-C3N4the/RGO composite photocatalyst.
TEM spectra of the product of example 1 according to the invention and further samples and EDS images of the product of example 1 according to the invention are shown in FIG. 2. Wherein (a) g-C3N4A TEM image of (B); (b) TEM image of RGO; (c) fe3O4@g-C3N4A TEM image of (B); (d) fe3O4@g-C3N4TEM image of/RGO; (e) fe3O4@g-C3N4EDS profile of/RGO. As can be seen from FIG. 2, pure g-C3N4The photocatalyst presents an irregular flaky shape; RGO is in the form of a super-lamellar; c shows Fe3O4Particle-forming nanowire-supported flake g-C3N4D is the layer g-C3N4The interlayer is spliced with sheet RGO, Fe3O4Nanowire loading in mutually staggered connected sheet-shaped g-C3N4And the upper surface of the platelet RGO.
The activity evaluation of the photodegradable tetracycline of the product of the example 1 and other samples is carried out according to the following method: the method is carried out in a D1 type photochemical reaction instrument (purchased from teaching instrument factories of Yangzhou university), 100 mL of 20 mg/L tetracycline simulation wastewater is added into a reaction bottle, magnetons and 0.05g of photocatalyst are added, a visible light power supply and an aeration device are opened for dynamic adsorption, and an external super constant temperature water bath is started to control the temperature of a reaction system to be 30 ℃. Performing light reaction after adsorption equilibrium is reached, sampling once every 15 minutes, centrifuging, measuring tetracycline concentration in supernatant, and passing through C/C0To judge the degradation effect of the tetracycline. Wherein, C0C is the tetracycline concentration at reaction time T. The results are shown in FIG. 3, in which (a) g-C3N4The degradation curve of (d); (b) fe3O4@g-C3N4Degradation curves for/RGO.
From FIG. 3, Fe can be seen3O4@g-C3N4the/RGO composite catalyst has better effect of degrading tetracycline through photocatalysis.
The UV-Vis diagrams of the product of example 1 and other samples according to the invention are shown in FIG. 4. FIG. 4 (a) Fe3O4@g-C3N4/RGO；（b）Fe3O4@g-C3N4；（c）RGO；（d）g-C3N4. As can be seen from FIG. 4, g-C3N4The photocatalyst has stronger absorption in a visible light region; fe3O4@g-C3N4Exhibits strong visible light absorption in the visible light region, Fe3O4@g-C3N4the/RGO composite photocatalyst has stronger light absorption performance in a visible light region.
The PL and FL plots for the product of example 1 of the present invention and other samples are shown in fig. 5. In FIG. 5, A is PL diagram, wherein (a) g-C3N4，（b）Fe3O4@g-C3N4，（c）Fe3O4@g-C3N4/RGO; b is FL diagram, wherein (a) g-C3N4，（b）Fe3O4@g-C3N4、（c）Fe3O4@g-C3N4and/RGO. As can be seen in FIG. 5A, g-C3N4Higher peak, indicating higher electron-hole recombination rate, and Fe3O4@g-C3N4the/RGO peak value is lower, which shows that the electron hole recombination rate is lower, and photo-generated electron holes can be fully utilized; fe can be seen in FIG. 5B3O4@g-C3N4The fluorescence lifetime of/RGO is long, the photo-generated electron and hole pair have better separation, which shows that the generated electron and hole are better utilized, and the photocatalytic activity is enhanced.
The VSM and cycle degradation profiles for the product of example 1 of the present invention and other samples are shown in figure 6. Wherein A is Fe3O4@g-C3N4And Fe3O4@g-C3N4VSM of/RGO, and Fe as the inset image3O4@g-C3N4/RGO; b is Fe3O4@g-C3N4Cyclic degradation profile of/RGO.
Fe is shown in FIG. 6A3O4@g-C3N4And Fe3O4@g-C3N4the/RGO composite photocatalyst shows better magnetism, but Fe3O4@g-C3N4the/RGO composite photocatalyst has better effect, and Fe can be seen in the inset3O4@g-C3N4the/RGO is easily separated by the applied magnetic field. From FIG. 6B, Fe3O4@g-C3N4the/RGO composite photocatalyst still has good catalytic effect after 5 times of circulation experiments.
Claims (1)
1. Fe3O4@g-C3N4Preparation method of/RGO composite photocatalyst in layered g-C3N4Between which is inserted a sheet-like RGO at g-C3N4And the upper surface of RGO is loaded with Fe3O4The nano-wire formed by the particles is characterized by comprising the following steps in sequence:
a. preparation of g-C3N4Pulverizing;
b. g to C3N4Dispersing the powder in ethylene glycol, keeping ultrasonic magnetic stirring in a water bath, then adding ferric nitrate nonahydrate, sodium acetate, polyethylene glycol 4000 and polyvinylpyrrolidone, continuing ultrasonic stirring, and then adding redox graphene until the added raw materials are uniformly dispersed or dissolved to obtain a dispersion liquid; the g to C3N4The dosage ratio of the ethylene glycol, the ferric nitrate nonahydrate, the sodium acetate, the polyethylene glycol 4000, the polyvinylpyrrolidone and the redox graphene is 0.1-1.0 g: 10-60 mL: 0.02-0.4 g: 0.02-0.4 g: 0.003-0.04 g: 0.0005-0.008 g: 0.005g to 0.015 g;
c. putting the obtained dispersion liquid into a hydrothermal kettle, and reacting for 10-15 h at 180-220 ℃;
d. cooling to room temperature, collecting solid product, washing and drying to obtain Fe3O4@g-C3N4the/RGO composite photocatalyst.
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| CN110465316A (en) * | 2018-10-17 | 2019-11-19 | 黑龙江大学 | A kind of photochemical catalyst g-C3N4/ GO composite material and preparation method |
| CN110465317A (en) * | 2018-10-18 | 2019-11-19 | 黑龙江大学 | A kind of photochemical catalyst g-C3N4/ GO/ magnetic particle and preparation method thereof |
| CN109317181A (en) * | 2018-11-02 | 2019-02-12 | 平顶山学院 | A kind of ferroferric oxide/carbon/carbon nitride material and its manufacturing method and purposes |
| CN110252372A (en) * | 2019-05-31 | 2019-09-20 | 江苏大学 | A kind of two dimension rGO/R-CeO2The preparation method of/CNNS hierarchical structure composite photo-catalyst |
| CN110280295A (en) * | 2019-07-19 | 2019-09-27 | 盐城工学院 | A kind of g-C3N4Base composite photocatalyst material and preparation method thereof |
| CN111266126B (en) * | 2020-02-25 | 2022-08-19 | 同济大学 | Preparation method and application of sulfur-doped graphite-phase carbon nitride nanosheet-loaded graphene and ferroferric oxide composite magnetic photocatalyst |
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